# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Zhaomin Hou'
_publ_contact_author_address     
;
Organometallic Chemistry Lab
RIKEN
Hirosawa 2-1
Wako
Saitama
351-0198
JAPAN
;

_publ_contact_author_email       HOUZ@RIKEN.JP

_publ_section_title              
;
Alkali-Metal-Catalyzed Addition of Primary and
Secondary Phosphines to Carbodiimides. A General and Efficient Route to
Substituted Phosphaguanidines
;
loop_
_publ_author_name
'Zhaomin Hou.'
'Masayoshi Nishiura'
'Wen-Xiong Zhang.'

# Attachment '2.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 606651'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H42 K N2 O P'
_chemical_formula_weight         504.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.1009(12)
_cell_length_b                   19.529(2)
_cell_length_c                   14.3917(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.539(2)
_cell_angle_gamma                90.00
_cell_volume                     2881.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14823
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.05
_reflns_number_total             5091
_reflns_number_gt                3848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0664P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5091
_refine_ls_number_parameters     305
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1716
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.07606(6) 0.06795(3) -0.01215(4) 0.0438(2) Uani 1 1 d . . .
P1 P 0.12339(6) 0.07294(3) 0.32734(5) 0.0336(2) Uani 1 1 d . . .
N1 N -0.0490(2) 0.05319(12) 0.12975(15) 0.0397(5) Uani 1 1 d . . .
N2 N 0.1374(2) -0.00714(11) 0.16241(14) 0.0407(5) Uani 1 1 d . . .
O1 O 0.1664(6) 0.18227(15) -0.0652(3) 0.167(2) Uani 1 1 d . . .
C1 C 0.0674(2) 0.03360(12) 0.19516(17) 0.0330(5) Uani 1 1 d . . .
C2 C -0.1377(2) 0.09649(14) 0.15611(18) 0.0373(6) Uani 1 1 d . . .
H2 H -0.1127 0.0952 0.2292 0.045 Uiso 1 1 d R . .
C3 C -0.1329(3) 0.17050(14) 0.1243(2) 0.0514(7) Uani 1 1 d . . .
H3A H -0.1486 0.1718 0.0532 0.062 Uiso 1 1 calc R . .
H3B H -0.0465 0.1889 0.1611 0.062 Uiso 1 1 calc R . .
C4 C -0.2338(3) 0.21530(16) 0.1435(3) 0.0631(9) Uani 1 1 d . . .
H4A H -0.2132 0.2178 0.2153 0.076 Uiso 1 1 calc R . .
H4B H -0.2301 0.2613 0.1194 0.076 Uiso 1 1 calc R . .
C5 C -0.3691(3) 0.18715(16) 0.0913(3) 0.0580(8) Uani 1 1 d . . .
H5A H -0.3925 0.1880 0.0191 0.070 Uiso 1 1 calc R . .
H5B H -0.4308 0.2156 0.1066 0.070 Uiso 1 1 calc R . .
C6 C -0.3769(3) 0.11433(16) 0.1249(3) 0.0548(8) Uani 1 1 d . . .
H6A H -0.4636 0.0962 0.0882 0.066 Uiso 1 1 calc R . .
H6B H -0.3611 0.1139 0.1960 0.066 Uiso 1 1 calc R . .
C7 C -0.2757(3) 0.06941(14) 0.1058(2) 0.0468(7) Uani 1 1 d . . .
H7A H -0.2795 0.0235 0.1304 0.056 Uiso 1 1 calc R . .
H7B H -0.2976 0.0664 0.0339 0.056 Uiso 1 1 calc R . .
C8 C 0.2618(2) -0.03698(13) 0.22426(18) 0.0349(6) Uani 1 1 d . . .
H8 H 0.2794 -0.0285 0.2954 0.042 Uiso 1 1 d R . .
C9 C 0.2548(3) -0.11454(13) 0.2048(2) 0.0429(6) Uani 1 1 d . . .
H9A H 0.1883 -0.1341 0.2250 0.051 Uiso 1 1 calc R . .
H9B H 0.2286 -0.1225 0.1332 0.051 Uiso 1 1 calc R . .
C10 C 0.3827(3) -0.15093(14) 0.2603(2) 0.0502(7) Uani 1 1 d . . .
H10A H 0.4038 -0.1481 0.3322 0.060 Uiso 1 1 calc R . .
H10B H 0.3737 -0.1989 0.2416 0.060 Uiso 1 1 calc R . .
C11 C 0.4924(3) -0.11996(15) 0.2368(2) 0.0530(7) Uani 1 1 d . . .
H11A H 0.4778 -0.1289 0.1670 0.064 Uiso 1 1 calc R . .
H11B H 0.5741 -0.1414 0.2785 0.064 Uiso 1 1 calc R . .
C12 C 0.5020(3) -0.04271(15) 0.2555(2) 0.0470(7) Uani 1 1 d . . .
H12A H 0.5283 -0.0340 0.3269 0.056 Uiso 1 1 calc R . .
H12B H 0.5681 -0.0237 0.2343 0.056 Uiso 1 1 calc R . .
C13 C 0.3723(3) -0.00747(13) 0.19840(19) 0.0396(6) Uani 1 1 d . . .
H13A H 0.3506 -0.0123 0.1267 0.047 Uiso 1 1 calc R . .
H13B H 0.3808 0.0410 0.2142 0.047 Uiso 1 1 calc R . .
C14 C 0.1410(2) 0.00092(13) 0.41303(18) 0.0357(6) Uani 1 1 d . . .
C15 C 0.1768(3) 0.01495(15) 0.51557(19) 0.0425(6) Uani 1 1 d . . .
H15 H 0.2022 0.0591 0.5392 0.051 Uiso 1 1 calc R . .
C16 C 0.1750(3) -0.03546(17) 0.5822(2) 0.0494(7) Uani 1 1 d . . .
H16 H 0.2004 -0.0253 0.6502 0.059 Uiso 1 1 calc R . .
C17 C 0.1357(3) -0.10053(17) 0.5482(2) 0.0521(7) Uani 1 1 d . . .
H17 H 0.1336 -0.1345 0.5929 0.062 Uiso 1 1 calc R . .
C18 C 0.0993(3) -0.11539(16) 0.4473(2) 0.0531(8) Uani 1 1 d . . .
H18 H 0.0724 -0.1595 0.4241 0.064 Uiso 1 1 calc R . .
C19 C 0.1027(3) -0.06498(13) 0.3804(2) 0.0431(6) Uani 1 1 d . . .
H19 H 0.0788 -0.0757 0.3127 0.052 Uiso 1 1 calc R . .
C20 C 0.2891(2) 0.10202(12) 0.35005(18) 0.0346(6) Uani 1 1 d . . .
C21 C 0.2998(3) 0.15425(13) 0.2875(2) 0.0449(7) Uani 1 1 d . . .
H21 H 0.2254 0.1696 0.2350 0.054 Uiso 1 1 calc R . .
C22 C 0.4190(3) 0.18350(14) 0.3022(2) 0.0522(7) Uani 1 1 d . . .
H22 H 0.4238 0.2182 0.2594 0.063 Uiso 1 1 calc R . .
C23 C 0.5311(3) 0.16179(15) 0.3797(2) 0.0542(8) Uani 1 1 d . . .
H23 H 0.6112 0.1816 0.3894 0.065 Uiso 1 1 calc R . .
C24 C 0.5224(3) 0.11026(15) 0.4427(2) 0.0487(7) Uani 1 1 d . . .
H24 H 0.5973 0.0951 0.4949 0.058 Uiso 1 1 calc R . .
C25 C 0.4028(3) 0.08093(14) 0.42849(19) 0.0411(6) Uani 1 1 d . . .
H25 H 0.3984 0.0467 0.4720 0.049 Uiso 1 1 calc R . .
C26 C 0.2801(9) 0.1525(4) -0.1061(7) 0.079(2) Uiso 0.50 1 d P . .
C27 C 0.1983(5) 0.1262(4) -0.1951(4) 0.133(2) Uani 1 1 d . . .
C28 C 0.2474(12) 0.2421(7) -0.0014(10) 0.128(4) Uiso 0.50 1 d P . .
C29 C 0.1693(7) 0.2709(3) 0.0385(4) 0.137(2) Uani 1 1 d . . .
C30 C 0.1583(11) 0.1904(6) -0.1658(8) 0.108(3) Uiso 0.50 1 d P . .
C31 C 0.0933(10) 0.2485(5) -0.0510(8) 0.102(3) Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0489(4) 0.0469(4) 0.0389(4) -0.0020(2) 0.0206(3) -0.0082(3)
P1 0.0330(4) 0.0403(4) 0.0277(3) -0.0028(2) 0.0118(3) 0.0021(3)
N1 0.0337(11) 0.0548(13) 0.0295(11) -0.0052(9) 0.0108(9) 0.0089(10)
N2 0.0381(12) 0.0528(13) 0.0298(11) -0.0043(9) 0.0117(9) 0.0100(10)
O1 0.353(7) 0.0503(16) 0.157(3) -0.0250(19) 0.162(4) -0.046(3)
C1 0.0354(13) 0.0382(13) 0.0267(12) -0.0015(10) 0.0132(11) 0.0001(11)
C2 0.0341(14) 0.0501(15) 0.0285(12) -0.0016(11) 0.0128(11) 0.0067(12)
C3 0.0455(17) 0.0487(17) 0.0644(19) -0.0047(14) 0.0258(15) -0.0011(13)
C4 0.059(2) 0.0486(18) 0.085(2) -0.0048(16) 0.0312(18) 0.0066(15)
C5 0.0483(18) 0.0587(19) 0.0642(19) -0.0009(15) 0.0185(16) 0.0174(15)
C6 0.0349(15) 0.0639(19) 0.0666(19) -0.0036(15) 0.0206(14) 0.0056(14)
C7 0.0371(15) 0.0478(16) 0.0555(17) -0.0016(12) 0.0177(13) 0.0036(12)
C8 0.0351(14) 0.0398(14) 0.0306(13) -0.0038(10) 0.0137(11) 0.0042(11)
C9 0.0422(15) 0.0433(15) 0.0481(15) -0.0084(12) 0.0227(13) -0.0022(12)
C10 0.0522(17) 0.0421(15) 0.0602(18) 0.0027(13) 0.0260(15) 0.0095(13)
C11 0.0451(17) 0.0525(17) 0.0631(19) 0.0001(14) 0.0228(15) 0.0136(14)
C12 0.0364(15) 0.0541(17) 0.0525(16) -0.0031(13) 0.0189(13) 0.0006(13)
C13 0.0433(15) 0.0411(14) 0.0379(13) -0.0005(11) 0.0196(12) 0.0034(12)
C14 0.0288(13) 0.0483(15) 0.0334(13) 0.0004(11) 0.0159(11) 0.0026(11)
C15 0.0356(14) 0.0575(17) 0.0347(13) -0.0018(12) 0.0137(12) -0.0041(12)
C16 0.0380(15) 0.076(2) 0.0335(14) 0.0073(13) 0.0133(12) -0.0044(14)
C17 0.0463(16) 0.0657(19) 0.0520(17) 0.0184(15) 0.0276(14) 0.0014(15)
C18 0.0556(18) 0.0494(17) 0.067(2) 0.0009(14) 0.0370(16) -0.0059(14)
C19 0.0453(16) 0.0490(16) 0.0418(15) -0.0061(12) 0.0243(13) -0.0051(12)
C20 0.0365(13) 0.0360(13) 0.0326(12) -0.0050(10) 0.0150(11) 0.0011(11)
C21 0.0436(16) 0.0432(15) 0.0467(16) 0.0054(12) 0.0158(13) 0.0033(12)
C22 0.0575(19) 0.0405(15) 0.0638(19) 0.0082(13) 0.0291(16) -0.0021(14)
C23 0.0420(16) 0.0527(18) 0.069(2) -0.0084(15) 0.0221(15) -0.0097(14)
C24 0.0350(15) 0.0578(18) 0.0488(16) -0.0056(14) 0.0111(13) -0.0013(13)
C25 0.0392(15) 0.0483(15) 0.0360(14) -0.0006(11) 0.0147(12) -0.0014(12)
C27 0.093(4) 0.207(7) 0.124(4) -0.008(4) 0.068(4) -0.019(4)
C29 0.195(6) 0.120(4) 0.104(4) 0.013(3) 0.066(4) 0.066(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O1 2.676(3) . ?
K1 N2 2.759(2) . ?
K1 N2 2.788(2) 3 ?
K1 N1 2.857(2) 3 ?
K1 N1 2.891(2) . ?
K1 C1 3.095(2) . ?
K1 C1 3.192(2) 3 ?
K1 K1 3.2357(12) 3 ?
P1 C14 1.831(3) . ?
P1 C20 1.831(3) . ?
P1 C1 1.921(2) . ?
N1 C1 1.331(3) . ?
N1 C2 1.454(3) . ?
N1 K1 2.857(2) 3 ?
N2 C1 1.319(3) . ?
N2 C8 1.448(3) . ?
N2 K1 2.788(2) 3 ?
O1 C30 1.424(11) . ?
O1 C28 1.544(13) . ?
O1 C31 1.580(11) . ?
O1 C26 1.688(9) . ?
C1 K1 3.192(2) 3 ?
C2 C7 1.516(4) . ?
C2 C3 1.523(4) . ?
C3 C4 1.527(4) . ?
C4 C5 1.503(5) . ?
C5 C6 1.515(4) . ?
C6 C7 1.532(4) . ?
C8 C13 1.524(3) . ?
C8 C9 1.537(4) . ?
C9 C10 1.514(4) . ?
C10 C11 1.510(4) . ?
C11 C12 1.529(4) . ?
C12 C13 1.521(4) . ?
C14 C19 1.380(4) . ?
C14 C15 1.400(3) . ?
C15 C16 1.380(4) . ?
C16 C17 1.372(4) . ?
C17 C18 1.380(4) . ?
C18 C19 1.388(4) . ?
C20 C25 1.394(3) . ?
C20 C21 1.395(4) . ?
C21 C22 1.381(4) . ?
C22 C23 1.382(4) . ?
C23 C24 1.382(4) . ?
C24 C25 1.387(4) . ?
C26 C27 1.355(10) . ?
C26 C30 1.491(13) . ?
C27 C30 1.445(12) . ?
C28 C29 1.334(13) . ?
C28 C31 1.586(15) . ?
C29 C31 1.315(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 K1 N2 135.61(12) . . ?
O1 K1 N2 115.72(12) . 3 ?
N2 K1 N2 108.64(5) . 3 ?
O1 K1 N1 119.18(9) . 3 ?
N2 K1 N1 91.86(6) . 3 ?
N2 K1 N1 47.37(6) 3 3 ?
O1 K1 N1 128.24(9) . . ?
N2 K1 N1 47.27(6) . . ?
N2 K1 N1 90.57(6) 3 . ?
N1 K1 N1 111.48(5) 3 . ?
O1 K1 C1 127.55(9) . . ?
N2 K1 C1 25.20(6) . . ?
N2 K1 C1 108.92(7) 3 . ?
N1 K1 C1 110.89(7) 3 . ?
N1 K1 C1 25.39(6) . . ?
O1 K1 C1 113.94(10) . 3 ?
N2 K1 C1 106.98(6) . 3 ?
N2 K1 C1 24.29(6) 3 3 ?
N1 K1 C1 24.62(6) 3 3 ?
N1 K1 C1 107.34(6) . 3 ?
C1 K1 C1 118.08(5) . 3 ?
O1 K1 K1 169.53(12) . 3 ?
N2 K1 K1 54.73(5) . 3 ?
N2 K1 K1 53.91(5) 3 3 ?
N1 K1 K1 56.23(5) 3 3 ?
N1 K1 K1 55.25(5) . 3 ?
C1 K1 K1 60.51(5) . 3 ?
C1 K1 K1 57.56(5) 3 3 ?
C14 P1 C20 106.11(11) . . ?
C14 P1 C1 105.68(11) . . ?
C20 P1 C1 102.84(11) . . ?
C1 N1 C2 123.6(2) . . ?
C1 N1 K1 91.95(14) . 3 ?
C2 N1 K1 135.09(16) . 3 ?
C1 N1 K1 85.93(14) . . ?
C2 N1 K1 133.07(16) . . ?
K1 N1 K1 68.52(5) 3 . ?
C1 N2 C8 125.2(2) . . ?
C1 N2 K1 91.79(14) . . ?
C8 N2 K1 128.15(15) . . ?
C1 N2 K1 95.30(15) . 3 ?
C8 N2 K1 129.21(15) . 3 ?
K1 N2 K1 71.36(5) . 3 ?
C30 O1 C28 108.4(7) . . ?
C30 O1 C31 101.8(7) . . ?
C28 O1 C31 61.0(6) . . ?
C30 O1 C26 56.5(5) . . ?
C28 O1 C26 97.2(7) . . ?
C31 O1 C26 144.7(5) . . ?
C30 O1 K1 119.9(5) . . ?
C28 O1 K1 131.2(5) . . ?
C31 O1 K1 112.2(4) . . ?
C26 O1 K1 103.0(3) . . ?
N2 C1 N1 117.8(2) . . ?
N2 C1 P1 125.74(18) . . ?
N1 C1 P1 116.32(17) . . ?
N2 C1 K1 63.00(12) . . ?
N1 C1 K1 68.68(13) . . ?
P1 C1 K1 138.61(11) . . ?
N2 C1 K1 60.41(13) . 3 ?
N1 C1 K1 63.43(13) . 3 ?
P1 C1 K1 159.29(11) . 3 ?
K1 C1 K1 61.92(5) . 3 ?
N1 C2 C7 109.5(2) . . ?
N1 C2 C3 111.6(2) . . ?
C7 C2 C3 109.4(2) . . ?
C2 C3 C4 112.1(2) . . ?
C5 C4 C3 111.2(3) . . ?
C4 C5 C6 110.6(3) . . ?
C5 C6 C7 110.2(3) . . ?
C2 C7 C6 113.0(2) . . ?
N2 C8 C13 111.4(2) . . ?
N2 C8 C9 108.3(2) . . ?
C13 C8 C9 108.51(19) . . ?
C10 C9 C8 113.2(2) . . ?
C11 C10 C9 111.6(2) . . ?
C10 C11 C12 111.3(2) . . ?
C13 C12 C11 111.3(2) . . ?
C12 C13 C8 112.4(2) . . ?
C19 C14 C15 117.9(2) . . ?
C19 C14 P1 123.20(19) . . ?
C15 C14 P1 118.3(2) . . ?
C16 C15 C14 121.2(3) . . ?
C17 C16 C15 120.0(3) . . ?
C16 C17 C18 119.7(3) . . ?
C17 C18 C19 120.4(3) . . ?
C14 C19 C18 120.8(3) . . ?
C25 C20 C21 117.6(2) . . ?
C25 C20 P1 126.0(2) . . ?
C21 C20 P1 116.1(2) . . ?
C22 C21 C20 121.1(3) . . ?
C21 C22 C23 120.7(3) . . ?
C24 C23 C22 119.0(3) . . ?
C23 C24 C25 120.5(3) . . ?
C24 C25 C20 121.0(3) . . ?
C27 C26 C30 60.8(6) . . ?
C27 C26 O1 98.1(6) . . ?
C30 C26 O1 52.8(5) . . ?
C26 C27 C30 64.2(6) . . ?
C29 C28 O1 104.3(9) . . ?
C29 C28 C31 52.7(6) . . ?
O1 C28 C31 60.6(6) . . ?
C31 C29 C28 73.5(7) . . ?
O1 C30 C27 107.1(8) . . ?
O1 C30 C26 70.7(6) . . ?
C27 C30 C26 55.0(6) . . ?
C29 C31 O1 103.3(7) . . ?
C29 C31 C28 53.8(6) . . ?
O1 C31 C28 58.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.091